JP3830008B2 - Non-aqueous electrolyte battery - Google Patents

Non-aqueous electrolyte battery Download PDF

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Publication number
JP3830008B2
JP3830008B2 JP31148098A JP31148098A JP3830008B2 JP 3830008 B2 JP3830008 B2 JP 3830008B2 JP 31148098 A JP31148098 A JP 31148098A JP 31148098 A JP31148098 A JP 31148098A JP 3830008 B2 JP3830008 B2 JP 3830008B2
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Prior art keywords
layer
material
electrolyte battery
battery according
nonaqueous electrolyte
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Expired - Lifetime
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JP31148098A
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JP2000138039A (en
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富太郎 原
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ソニー株式会社
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/056Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0565Polymeric materials, e.g. gel-type or solid-type
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2/00Constructional details or processes of manufacture of the non-active parts
    • H01M2/02Cases, jackets or wrappings
    • H01M2/0202Cases, jackets or wrappings for small-sized cells or batteries, e.g. miniature battery or power cells, batteries or cells for portable equipment
    • H01M2/0207Flat-shaped cells or batteries of flat cells
    • H01M2/0212Flat-shaped cells or batteries of flat cells with plate-like or sheet-like terminals
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2/00Constructional details or processes of manufacture of the non-active parts
    • H01M2/02Cases, jackets or wrappings
    • H01M2/0257Cases, jackets or wrappings characterised by the material
    • H01M2/0267Cases, jackets or wrappings characterised by the material of wrappings, outside coatings, jackets around completely closed cell elements
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2/00Constructional details or processes of manufacture of the non-active parts
    • H01M2/02Cases, jackets or wrappings
    • H01M2/0257Cases, jackets or wrappings characterised by the material
    • H01M2/0275Cases, jackets or wrappings characterised by the material of flexible envelopes or bags around open cell elements

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a nonaqueous electrolyte battery in which a unit cell is accommodated in an encapsulant made of a laminate film.
[0002]
[Prior art]
In recent years, electronic devices such as mobile phones and notebook computers have become cordless and portable, and thin, small, and lightweight portable electronic devices have been developed one after another. In addition, the amount of power used has increased due to diversification of devices, and there has been an increasing demand for higher capacities of batteries, particularly secondary batteries, which are energy sources for these electronic devices.
[0003]
Secondary batteries that have been used conventionally include lead-acid batteries and nickel-cadmium batteries, and nickel-hydrogen batteries and lithium-ion batteries have been put to practical use as new secondary batteries. However, since these secondary batteries use liquid as an electrolyte, there is a problem of leakage from the battery.
[0004]
Therefore, a polymer lithium ion secondary battery using a polymer gel swollen by an electrolyte as an electrolyte has been developed to solve such problems. With the development of this polymer lithium ion secondary battery, there is no risk of liquid leakage from the battery, and a secondary battery that is small, light, thin, and has a high energy density can be realized.
[0005]
The configuration of the polymer lithium ion secondary battery will be described. For example, an active material made of LiCoO 2 and graphite is laminated on a positive electrode current collector made of an aluminum thin plate, and carbon is placed on the negative electrode current collector made of a copper thin plate. , Coke, graphite and other active materials are laminated to form an electrode. A separator, which is a thin film having pores, is sandwiched between polypropylene, polyethylene, and the like, and between these electrodes and separators, such as polyacrylonitrile (PAN), polyethylene oxide (PEO), and polyvinylidene fluoride (PVDF). It has a sandwich structure filled with various polymer gel electrolytes.
[0006]
These unit cells (unit cells) having a sandwich structure are packaged with an encapsulant made of a metal thin film such as an aluminum foil and a plastic film such as nylon, polyethylene, polypropylene, or polyethylene terephthalate as an encapsulating container. .
[0007]
[Problems to be solved by the invention]
In general, since this type of battery is mounted in a small space of an electronic device in which parts are highly integrated, it is desirable to use a packaging material that is highly flexible against any stress. We have already developed a method for producing a card type battery in which an element is encapsulated with a flexible encapsulant while maintaining battery characteristics (see Japanese Patent Laid-Open No. 8-83596).
[0008]
Japanese Patent Application Laid-Open No. 9-288996 discloses a technique for improving the electrolyte sealing property by providing an insulating layer having an excellent electrolyte barrier property between the innermost heat-seal plastic layer and the metal layer of the sealing bag. Is disclosed.
[0009]
However, as the layer structure of the encapsulant becomes multi-layered as in the method described in Japanese Patent Laid-Open No. 9-288996 , for example, gas intrusion from the adhesion interface of each layer, separation of the interface adhesion part, etc. Reliability tends to be lower.
[0010]
Further, since an adhesive layer of at least 5 microns or more is required to bond each layer, the entire film thickness is increased, and as a result, the amount of gas permeation from the entire inner layer is increased.
[0011]
Therefore, it has been desired to develop a material for battery encapsulating material that has high sealing performance and adhesion and is thin.
[0012]
The present invention has been proposed in view of such conventional circumstances, and has an object to provide a battery encapsulating material that has high sealing performance and adhesion and is thin, thereby improving reliability. An object of the present invention is to provide a non-aqueous electrolyte battery that is high and can be made thinner.
[0013]
[Means for Solving the Problems]
As a result of diligent research to solve the above problems, the present inventors have obtained a sealing material having high sealing reliability by giving a characteristic to a plastic material that forms a layer inside the metal layer of the sealing material. I found out that
[0014]
The present invention has been completed based on such knowledge, and in a nonaqueous electrolyte battery in which a unit cell is accommodated in an encapsulant made of a laminate film, the encapsulant includes at least a metal layer and an inner side of the encapsulant. The heat fusion layer is composed of a plurality of material layers including the same monomer unit. That is, the thermal fusion layer includes a first material layer containing polypropylene and a second material layer containing a propylene copolymer provided on the side in contact with the metal layer, and the first material. A mixed region in which polypropylene and a propylene copolymer are mixed is provided between the layer and the second material layer.
[0015]
The encapsulating material described in the present invention has a multi-layer structure even though the adhesive layer is not present in the layer inside the metal foil portion. That is, the inner layer is made of a plastic material having a continuous layer structure rather than the metal foil layer. The continuous layer structure is composed of materials that have similar molecular skeletons, such as homopolymers and copolymers, and that can be chemically bonded or mixed, and form a layer structure that is difficult to peel off by physical means. ing. The materials forming the layer structure have different physical properties. For example, by combining a material with excellent electrolytic solution resistance and a material with excellent heat-fusibility, excellent sealing performance can be realized. Is possible.
[0016]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the configuration of a nonaqueous electrolyte battery to which the present invention is applied will be described with reference to the drawings.
[0017]
The nonaqueous electrolyte battery of the present invention is, for example, a solid electrolyte battery or a gel electrolyte battery. As shown in FIGS. 1 and 2, the solid electrolyte or gel is interposed between the positive electrode active material layer and the negative electrode active material layer. The unit cell 1 in which the electrolyte is disposed is housed in an encapsulant 2 made of a laminate film, and the surroundings are sealed by heat welding.
[0018]
The unit cell 1 is provided with a negative terminal lead 3 electrically connected to the negative electrode constituting the unit cell 1 and a positive terminal lead 4 electrically connected to the positive electrode. The positive terminal lead 4 is drawn out of the encapsulant 2.
[0019]
The encapsulant 2 used in the present invention has a structure in which plastic films 22 and 23 are bonded to a metal thin film 21 as shown in FIG. 3, for example. It is intended to be sealed by thermal fusion when the battery 1 is encapsulated, and corresponds to a thermal fusion layer.
[0020]
The plastic film 23 which is the outermost layer is preferably made of a plastic material excellent in strength such as nylon or polyethylene terephthalate (PET), and the thickness of the plastic film 23 can be reduced if the corrosion of the metal foil portion can be prevented and the strength of the encapsulant can be maintained. Although it does not matter, for example, nylon preferably has a thickness of 30 μm or more. Although the metal thin film 21 is made of a metal material having excellent gas permeability such as aluminum, the thickness of the metal thin film 21 is preferably 25 μm or more in order to maintain sufficient gas permeability.
[0021]
The plastic film 22 that forms the layer inside the metal thin film 21 is made of a plastic material having the same monomer unit as the skeleton. By having the same monomer unit in the skeleton, the affinity of the interface between the plastic materials is increased, and it is possible to form a continuous layer by a simple process such as heat fusion without using an adhesive. .
[0022]
In order to maintain the sealing property of the battery, at least one layer having excellent gas permeation resistance and one having excellent heat fusion property are required for the layer 22 inside the metal thin film 21. For this reason, in at least one kind of plastic material forming a multilayer structure, when a film having a thickness of 25 μm is placed in an environment of a temperature of 40 ° C. and a relative humidity of 90% for 24 hours, the water vapor transmission rate is 10 g / m 2. The following plastic materials are preferable, and the value is more preferably 6 g / m 2 or less. Further, in at least one kind of plastic material forming the multilayer structure, the dynamic viscoelasticity within the range of 5 ° C. or less from the melting point of the material is preferably 15% or less, and 13% or less. It is more preferable. If the material has a dynamic viscoelasticity lower than that or exhibits a fracture behavior, the degree of fusion is poor and the reliability of the battery in sealing performance is lowered. If it is more than that, the resin may flow and the layer structure of the heat-sealed portion may be destroyed.
[0023]
FIG. 4 schematically shows the structure of the plastic film 22, and a mixed region 22c in which the plastic materials constituting the material layers 22a and 22b are mixed is formed between the plurality of material layers 22a and 22b. The plastic film 22 is a continuous film having no clear interface.
[0024]
Here, the material layer 22a located in the innermost layer is made of, for example, a material having a dynamic viscoelasticity of 15% or less within the range of 5 ° C. from the melting point as described above. The opposite material layer 22b is made of a plastic material having a water vapor transmission rate of 10 g / m 2 or less when a film having a thickness of 25 μm is placed in an environment of a temperature of 40 ° C. and a relative humidity of 90% for 24 hours.
[0025]
As a plastic material satisfying the above items, a plastic material having polypropylene as a main skeleton is suitable, and a layer excellent in gas permeability is preferably a polyprolene homopolymer system having an average molecular weight of 150,000 or more. More preferably 180,000 or more. The layer excellent in heat-fusibility is a polypropylene copolymer type, and the copolymer component of the copolymer is preferably polyethylene, and the polyethylene content relative to polypropylene is preferably 3% by weight or more and 5% by weight or less. If the polyethylene content is higher than that, problems arise in terms of resistance to electrolytic solution and strength at the time of film formation, and if it is lower than that, the dynamic elastic modulus is not sufficiently lowered.
[0026]
On the other hand, when the unit cell 1 is a solid electrolyte battery or a gel electrolyte battery, for example, as a polymer material used for the polymer solid electrolyte, silicon gel, acrylic gel, acrylonitrile gel, polyphosphazene are used. Modified polymers, polyethylene oxide, polypropylene oxide, and their composite polymers, cross-linked polymers, modified polymers, etc., or fluorine-based polymers such as poly (vinylidene fluoride), poly (vinylidene fluoride-co-hexafluoropropylene), poly (Vinylidene fluoride-co-tetrafluoroethylene), poly (vinylidene fluoride-co-trifluoroethylene), and the like and various mixtures thereof can be used, but of course, the present invention is not limited thereto.
[0027]
For the solid electrolyte or gel electrolyte laminated on the positive electrode active material layer or the negative electrode active material layer, a solution comprising a polymer compound, an electrolyte salt, and a solvent (or a plasticizer in the case of a gel electrolyte) is used as the positive electrode active material. A layer or a negative electrode active material layer is impregnated, and the solvent is removed and solidified. Part of the solid electrolyte or the gel electrolyte laminated on the positive electrode active material layer or the negative electrode active material layer is impregnated into the positive electrode active material layer or the negative electrode active material layer to be solidified. In the case of a crosslinked system, it is then solidified by crosslinking with light or heat.
[0028]
The gel electrolyte is composed of a plasticizer containing a lithium salt and a matrix polymer of 2 wt% to 30 wt%. At this time, esters, ethers, carbonates and the like can be used alone or as one component of a plasticizer.
[0029]
In preparing the gel electrolyte, various polymers used to form the gel electrolyte can be used as the matrix polymer for gelling such carbonates. From the viewpoint of redox stability, For example, it is desirable to use a fluorine-based polymer such as poly (vinylidene fluoride) or poly (vinylidene fluoride-co-hexafluoropropylene).
[0030]
The polymer solid electrolyte is composed of a lithium salt and a polymer compound that dissolves the lithium salt. Examples of the polymer compound include ether polymers such as poly (ethylene oxide) and cross-linked polymers, poly (methacrylate) esters, and acrylates. Fluorine polymers such as poly (vinylidene fluoride) and poly (vinylidene fluoride-co-hexafluoropropylene) can be used singly or in combination. For example, poly (vinylidene) can be used because of redox stability. Fluoropolymers such as (fluoride) and poly (vinylidene fluoride-co-hexafluoropropylene) are preferably used.
[0031]
As a lithium salt to be contained in such a gel electrolyte or a polymer solid electrolyte, a lithium salt used in a normal battery electrolyte can be used. Examples of the lithium compound (salt) include the following. However, it is not limited to these.
[0032]
For example, lithium chloride lithium bromide, lithium iodide, lithium chlorate, lithium perchlorate, lithium bromate, lithium iodate, lithium nitrate, lithium tetrafluoroborate, lithium hexafluorophosphate, lithium acetate, bis (trifluoromethane Examples thereof include sulfonyl) imidolithium, LiAsF 6 , LiCF 3 SO 3 , LiC (SO 2 CF 3 ) 3 , LiAlCl 4 , and LiSiF 6 .
[0033]
These lithium compounds may be used alone or in combination, and among them, LiPF 6 and LiBF 4 are desirable from the viewpoint of oxidation stability.
[0034]
As a concentration for dissolving the lithium salt, a gel electrolyte can be used at 0.1 to 3.0 mol in the plasticizer, but preferably 0.5 to 2.0 mol / liter.
[0035]
The battery of the present invention can be configured in the same manner as a conventional lithium ion battery except that the gel electrolyte or solid electrolyte as described above is used.
[0036]
That is, as a negative electrode material for constituting a lithium ion battery, a material capable of doping and dedoping lithium can be used. A constituent material of such a negative electrode, for example, a non-graphitizable carbon material or a carbon material such as a graphite material can be used. More specifically, pyrolytic carbons, cokes (pitch coke, needle coke, petroleum coke), graphites, glassy carbons, organic polymer compound fired bodies (phenol resin, furan resin, etc.) at an appropriate temperature. Carbon materials such as those obtained by firing and carbonization), carbon fibers, activated carbon, and the like can be used. In addition, as a material capable of doping and dedoping lithium, a polymer such as polyacetylene or polypyrrole or an oxide such as SnO 2 can be used. In forming the negative electrode from such a material, a known binder or the like can be added.
[0037]
The positive electrode can be configured using a metal oxide, a metal sulfide, or a specific polymer as the positive electrode active material, depending on the type of the target battery. For example, in the case of constituting a lithium ion battery, the positive electrode active material may be a metal sulfide or oxide not containing lithium, such as TiS 2 , MoS 2 , NbSe 2 , V 2 O 5 , LiMO 2 (wherein M is one kind) The above transition metals are represented, and x varies depending on the charge / discharge state of the battery and is usually 0.05 or more and 1.10 or less. As the transition metal M constituting this lithium composite oxide, Co, Ni, Mn and the like are preferable. Specific examples of such a lithium composite oxide include LiCoO 2 , LiNiO 2 , LiNi y Co 1-y O 2 (where 0 <y <1), LiMn 2 O 4 and the like. . These lithium composite oxides can generate a high voltage and become a positive electrode active material excellent in energy density. A plurality of these positive electrode active materials may be used in combination for the positive electrode. Moreover, when forming a positive electrode using the above positive electrode active material, a well-known electrically conductive agent, a binder, etc. can be added.
[0038]
As the structure of the unit cell 1, a stacking type in which positive and negative electrodes are alternately stacked with a solid electrolyte sandwiched, a positive electrode and a negative electrode are stacked with a solid electrolyte sandwiched, and a winding type in which this is wound up, a positive electrode and a negative electrode Examples include a folding type in which the solid electrolytes are stacked and alternately folded, and can be arbitrarily selected.
[0039]
In addition, the present invention can be applied to both primary batteries and secondary batteries. However, when the present invention is applied to a non-aqueous electrolyte secondary battery, a great effect can be obtained.
[0040]
【Example】
Next, specific examples and comparative examples to which the present invention is applied will be described based on experimental results.
[0041]
The unit cell used for the evaluation is a sandwich structure in which the positive electrode is lithium cobalt oxide and graphite, the negative electrode is graphite, the positive electrode current collector is aluminum foil, the negative electrode current collector is copper foil, and the solid electrolyte is filled with polyvinylidene fluoride (PVDF). The outer dimensions of the unit cell are 5 cm × 4 cm × 0.4 cm, and the capacity is 450 mAh.
[0042]
This unit cell was encapsulated in each encapsulant so that the terminal could be taken out, and the side surface was sealed at 210 ° C., 3.5 kgf / cm 2 , and a seal width of 5 mm.
[0043]
In the encapsulating material, the first layer serving as the metal foil side layer was formed by stretching a polypropylene homopolymer (PP) having a number average molecular weight of 182,000 and a melting point of 160 ° C. to form a film having a thickness of 20 μm. The second layer, which is a fusion layer, was formed by drawing a polypropylene copolymer (CPP) having a number average molecular weight of 155,000, a melting point of 143 ° C., and a polyethylene content of 4% by weight into a film having a thickness of 12 μm. The two films formed in this manner are pressure-bonded at 200 ° C. and 5.0 kgf / cm 2 to form a continuous layer film (PP-CPP: thickness 30 μm) having virtually no film interface. It was done.
[0044]
The formed film (PP-CPP) was bonded to a 40 μm aluminum foil (Al) by an extrusion method, and similarly a 25 μm nylon film (Ny) was bonded to form an encapsulating material.
[0045]
By the same method, the structure of the exterior material was changed as shown in Table 1, and Samples 1 to 5 were produced. In Table 1, LDPE represents low density polyethylene, and PET represents polyethylene terephthalate.
[0046]
After the sample battery produced as described above was held in a thermostat at 70 ° C. for 500 hours, the volatilization amount of the electrolyte component and the water penetration amount were measured, and the peeling state of each layer was observed. The results are shown in Table 1.
[0047]
[Table 1]
[0048]
As is clear from Table 1, in Sample 1 corresponding to the example of the present invention, sufficient sealing performance is ensured even if the thickness of the exterior material is reduced, and the volatilization amount of the electrolyte component and the amount of moisture intrusion There is very little. Also, no interfacial delamination is observed.
[0049]
【The invention's effect】
As is clear from the above description, according to the present invention, it is possible to provide a thin non-aqueous electrolyte battery having high sealing properties and adhesiveness.
[Brief description of the drawings]
FIG. 1 is an exploded perspective view showing a configuration example of a solid electrolyte battery to which the present invention is applied.
FIG. 2 is a schematic perspective view showing a configuration example of a solid electrolyte battery to which the present invention is applied.
FIG. 3 is a cross-sectional view showing a configuration example of an exterior material.
FIG. 4 is a schematic cross-sectional view schematically showing a configuration example of a heat-fusible layer.
[Explanation of symbols]
1 unit cell, 2 exterior material, 3 negative terminal lead, 4 positive terminal lead, 21 metal thin film, 22 plastic film (heat fusion layer)

Claims (9)

  1. In a non-aqueous electrolyte battery in which a unit cell is housed in an encapsulant made of a laminate film,
    The encapsulant has at least a metal layer and a heat fusion layer disposed on the inner side of the metal layer,
    The heat-fusible layer includes a first material layer containing polypropylene and a second material layer containing a propylene copolymer provided on the side in contact with the metal layer, and the first material layer. A nonaqueous electrolyte battery comprising a mixed region in which polypropylene and a propylene copolymer are mixed between the first material layer and the second material layer .
  2. The nonaqueous electrolyte battery according to claim 1, wherein the thickness of the heat sealable layer is 20 to 40 [mu] m.
  3.   Of the material layers constituting the heat-sealing layer, the innermost material layer is made of a plastic material having a dynamic viscoelasticity of 15% or less within a range of 5 ° C. from the melting point. The nonaqueous electrolyte battery according to claim 1.
  4. The material layer constituting the fusion layer is made of a plastic material having a water vapor transmission rate of 10 g / m 2 or less when a 25 μm-thick film is placed in an environment of a temperature of 40 ° C. and a relative humidity of 90% for 24 hours. The nonaqueous electrolyte battery according to claim 1, further comprising a layer.
  5. The propylene copolymer is a non-aqueous electrolyte battery according to claim 1, wherein the containing ethylene as a copolymer component.
  6.   2. The nonaqueous electrolyte battery according to claim 1, wherein the electrolyte constituting the unit cell is a gel electrolyte or a solid electrolyte containing a matrix polymer and a lithium salt.
  7.   The nonaqueous electrolyte battery according to claim 1, wherein the negative electrode constituting the unit cell is a negative electrode containing a material capable of doping and dedoping lithium.
  8. 8. The nonaqueous electrolyte battery according to claim 7, wherein the material capable of doping and dedoping lithium is a carbon material.
  9.   The nonaqueous electrolyte battery according to claim 1, wherein the positive electrode constituting the unit cell is a positive electrode containing a composite oxide of lithium and a transition metal.
JP31148098A 1998-10-30 1998-10-30 Non-aqueous electrolyte battery Expired - Lifetime JP3830008B2 (en)

Priority Applications (1)

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JP31148098A JP3830008B2 (en) 1998-10-30 1998-10-30 Non-aqueous electrolyte battery

Applications Claiming Priority (7)

Application Number Priority Date Filing Date Title
JP31148098A JP3830008B2 (en) 1998-10-30 1998-10-30 Non-aqueous electrolyte battery
TW088118077A TW463412B (en) 1998-10-30 1999-10-19 Non-aqueous electrolyte cell
US09/422,251 US6296971B1 (en) 1998-10-30 1999-10-21 Non-aqueous electrolyte cell
CNB99123619XA CN1161855C (en) 1998-10-30 1999-10-29 Non liquid electrolyte battery
EP99121573A EP0997954B1 (en) 1998-10-30 1999-10-29 Non-aqueous electrolyte cell
DE69905437T DE69905437T2 (en) 1998-10-30 1999-10-29 Cell with non-aqueous electrolyte
KR1019990047685A KR100619652B1 (en) 1998-10-30 1999-10-30 Non-Aqueous Electrolyte Cell

Publications (2)

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JP2000138039A JP2000138039A (en) 2000-05-16
JP3830008B2 true JP3830008B2 (en) 2006-10-04

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US (1) US6296971B1 (en)
EP (1) EP0997954B1 (en)
JP (1) JP3830008B2 (en)
KR (1) KR100619652B1 (en)
CN (1) CN1161855C (en)
DE (1) DE69905437T2 (en)
TW (1) TW463412B (en)

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